Hydrochloric Acid → N-[2-(2-ethoxyethoxy)-phenyl-sulfonyl]-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)-urea

HRID 463956노트

반응식

HRID 463956 반응식
N12CCCCC1C=NCCC2.O([C:19]([NH:21][C:22]1[N:27]=[C:26]([O:28][CH:29]([F:31])[F:30])[CH:25]=[C:24]([CH3:32])[N:23]=1)=[O:20])C1C=CC=CC=1.[CH2:33]([O:35][CH2:36][CH2:37][O:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=1[S:45]([NH2:48])(=[O:47])=[O:46])[CH3:34].Cl>C(#N)C.O.C(OCC)(=O)C>[CH2:33]([O:35][CH2:36][CH2:37][O:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=1[S:45]([NH:48][C:19]([NH:21][C:22]1[N:27]=[C:26]([O:28][CH:29]([F:30])[F:31])[CH:25]=[C:24]([CH3:32])[N:23]=1)=[O:20])(=[O:46])=[O:47])[CH3:34]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 201856962-(Ethoxy-ethoxy)-benzenesulfonamideHCID 221041722-Phenoxycarbonylamino-4-difluoromethoxy-6-methyl-pyrimidine

생성물 1

HCID 53940140N-[2-(2-ethoxyethoxy)-phenyl-sulfonyl]-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)-urea

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

1.8 g (0.012 mol) of 1,5-diazabicyclo(5.4.0)undec-5-ene are added to a solution of 3.5 g (0.012 mol) of 2-phenoxycarbonylamino-4-difluoromethoxy-6-methyl-pyrimidine, in the form of the crude product, and 2.9 g (0.012 mol) of 2-(2-ethoxy-ethoxy)-benzenesulfonamide in 100 ml of absolute acetonitrile and the mixture is stirred at 20°-25° C. for 1 hour and then diluted with 500 ml of water and acidified with hydrochloric acid. The oil which separates out is taken up in 200 ml of ethyl acetate and the mixture is dried over sodium sulfate and evaporated. The oily residue is crystallised from diethyl ether and acetone to give N-[2-(2-ethoxyethoxy)-phenyl-sulfonyl]-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)-urea of melting point 90°-95° C. (decomposition) as colourless crystals in a yield of 2.7 g.

후처리

  1. dry with materialthe mixture is dried over sodium sulfate
  2. customevaporated
  3. customThe oily residue is crystallised from diethyl ether and acetone

출처 및 근거

ORD 기록
ord-1d8d00c21822438988832e16c516d814
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04545811

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